Process of saponifying glycerids.



BALTHASAR E. REUTER, or cnrcneo, ILLINOIS, ASSIGNOR '10 nnurnn raoonssCOMPANY, OF CHICAGO, ILLINOIS, A CORPORATION OIELILLINOIS.

No Drawing.

To all whom it may concern:

Be it known that I, BALTHAS'AR E. REUTER, a citizen of the UnitedStates, residin at Chicago, in the county of Cook and tate of Illinois,have invented a new and Imroved Process of Saponifying .Glycerids, ofwhichthefollowing is a specification.

This invention relates to an improvement in the art of s aponifyingglycerids with the aid of a saponifier, preferably a catalyticsaponifier, namely, such as is used in the process described in UnitedStates Patent No. 601,603, dated March 29, 1898, and its variousequivalent processes such as those of United States Patents No.1,082,662 of December 30, 1913., No. 1,058,633, of April 8,

esses are, as a rule,

.1913, and No.1,079,437 of November 25,1913.

The fatty acids resultingfrom such procrate, sufiiciently colored as torequire a subsequent cleansing treatment to render them useful for theproduction of white, or commercially white materials, stearic acid andsoaps.

I have found that this tendency to discolorization can be greatlyovercome, in a process such as that of United States Patent No. 601,603referred to, wherein the entire amount or substantially the entireamount of saponifier to be used is added directly to the material aboutto undergo saponification. I have discovered that by diminishing thelength of time of contact of the unsaponified material and of the fattyacid product of the saponification on the one hand, with the wateryportion of the mix.

and the dissolved products contained in the .fatty material, on theother hand, that this discolorization of the fatty acid product can bein a great measure reduced. Upon this discovery, I have based thefollowing invention, which in outline is, broadly, as follows:-I add tothe glycerid to be saponified, the total amount of saponifier,preferably catalytic saponifier, and the total amount of water, and thenecessary amount of mineral acid. I then boil for a period of time whichis a fraction of the entire required boiling period, for example,onethird, say twenty-four (24) hours; I then allow the result toseparate, assisting such separation, if necessary, by the use ofsulfuric acid and upon completed separation I withdraw the entire wateryportion to- Specification of Letters Patent.

highly colored, or at anysuch as candles,

PROCESS OF SAPONIFYING GLYCERIDS.

Patented Mar. 25, 1919.

App1ication filed April 9, 1914. Serial No. 830,590.

gether with any, and preferably all, of the dlscolored material whichseparates as what may be termed, a ribbon just above the watery layerand just below the unsaponified glycerld, and the fatty acid; thereupon,or concurrently, I separate the watery portion from the above referredtoribbon, return, preferably, the entire amount of watery materlal tothe 'saponification vessel, and '-proceed with the boiling for anotherperiod of, for example, twenty-four (24) hours. The

removal of the watery layer and the discol ored material is thenrepeated as before, and the watery layer when separated from thediscolored layer or ribbon is returned to the saponification vessel andthe saponification is then resumed and o It occasionally happens that itis well to, add a fraction say 10%, of the original amount of saponifierto the watery portion prior to one or more of .the successive boils; thesame effect can also be obtained by originally taking an additionalamount of the saponifier indicated, which additional amount is ingeneral to be suflicient to make up for the loss of saponifier removedwith the ribbon. As to the amount of such excess (usually. 15 to 25%) ofsaponifier, the operator must have some regard quality of the materialstaken for saponification and the relative or actual amount of the ribbonremoved. I illustrate this by means of the following example, which istaken from a factory operation; but my invention is not limited to thematerials or conditions herein used for the purposes of illustration.

Place 50,000 lbs. of glyeerid (consisting, for example, of equal partsof hydrolyzed fish oil and of summer yellow cottonseed oil) in asuitable saponifying apparatus, add thereto 33,000 lbs. of water, 150lbs. of sulfuric acid containing H,SO,, 300 lbs. of the naphthalenevariety of the Twitchell saponifier, (United States Patent No. 628,503of July 11, 1899) boil for twenty-four (24) hours; remove the ribbon andthe water; separate the water from the ribbon; return the water tothe-stock, and boil for another twenty-four (2 1) to the nature andcarried to completion.

' cient agitation.

the boil,the fatty acids are ready for use in the production of candles,stearlc acid. or soap. v

The results are 'improvedand made more certain of achievement,by'exclusion of air during the saponification combined with effi-Iclaim: 1 1. In the art of saponifylng glycerid the improvement which,comprises removal of the watery layer and discolored fatty mate materialbetween the watery and non-watery rial from the. saponifying apparatusand return of the watery portion freed fromthe discolored; fattymaterial.

2. The/process 'of 'saponifying glycerid which consists in bringingabout saponification and thereby forming a ribbon of colored contents ofthe apparatus and removing such colored ribbon from the saponifying ap-'.paratus.

3. which comprises adding to the glycerid water sulfuric acid andsaponifie'r; bringingabout saponification; interrupting said S3,",

' ponification'; removing the watery portion whichcomprises treating theand the discolored fatty portion of the contents of the saponifyingapparatus and returning to the saponifyin-g apparatusthe watery portionso removed and;resuming the saponifying operation.

4. The process of 'saponifying glycerid glycerid with water, acid andsaponifier, bringing about saponification, interrupting the saponifyingoperation, removing the colored material accompanying the non-wateryportion of the contents of the saponifying apparatus, and

resuming the saponifying operation.

5 The process of. saponifying glycerid which consists in bringing aboutsaponifica-- tion, interrupting the saponification, remov ing the waterylayer and discolored fatty material from the saponifying apparatus,

.acid, and saponifier to theglycerid under treatment, boiling themixture thus formed, interrupting, the boiling operation beforesaponlfication 1s completed, settling out the The process of saponifyingglycerid saponified glycerid and fattyajcid.

the saponifying opera- 7 tenal.

wateryv portion of the mixture by means of j cerid and fatty acid,separating the discolored material from the wateryeportion, returningthe watery portion to themixture, and resuming the boiling'operation. 9.The method which consists in successively performing the followingoperations: boiling a mixture'of glycerid, water, and saponifier, tionbefore sapo'nificationis completed, settling the watery portion'of themixture out of the'unsaponified glycerid and fatty acid, removing theribbon of discolored material which separates the watery portion fromthe unsaponified glycerid and fatty acid, and resuming the boilingoperation.

10. The method of 'saponifying glycerid which consists in successivelyheating a mixture of the glycerid under treatment, water, andsaponifier, settling out the watery portion of the mixture between eachheating of the mixture, and removing the discolored material between thewatery portion and un-' 11. The process ofsaponifying glycerid whicheonslsts inbringing aboutsaponification and thereby forming a ribbon ofcol ored material between the watery and non glycerid undertreatinterrupting the boiling operareturning the watery portion andresuming the boiling op v portion to settle out of the mixture,

watery contents of the'apparatus, removing I such colored ribbon fromthe sapomfying. apparatus and thereupon replenishing ,the mhtrgure undertreatment with a supply of wa r containing no discolored In testimonywhereof .I have hereunto my scribing witnesses.

fatty maname. in the presence of two sub- BALTHASAR E. REUTER.

Witnesses:

M. E. MCNINCH, E. Locxwoon.

